CN110918085A - 一种多孔wo3/c纳米片介孔复合光催化剂的制备方法 - Google Patents
一种多孔wo3/c纳米片介孔复合光催化剂的制备方法 Download PDFInfo
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Abstract
本发明提供了一种多孔WO3/C纳米片介孔复合光催化剂的制备方法,将有机胺插层WO3·2H2O的杂化物加入瓷舟中,然后放入管式炉中,通入氮气,加热升温,保温反应,反应完后自然冷却至室温,即得到多孔WO3/C纳米片介孔复合光催化剂材料。本发明方法制备的多孔WO3/C纳米片介孔复合光催化剂由C与多孔的WO3纳米片形成的介孔结构的复合材料,具有良好的光吸收性能和较大的比表面积,在光照下能够高效的转化氮气成硝酸根,具有较好的光催化氧化活性。
Description
技术领域
本发明所属技术领域为光催化、光电化学材料技术领域,特别涉及多孔WO3/C纳米片介孔复合光催化剂的制备方法。
背景技术
三氧化钨为一种宽禁带的n型半导体材料,室温下的禁带宽度为2.63eV,可吸收500nm以下的可见光及紫外光,在电致变色、气敏传感器、光催化与光电转换领域具有重要的应用价值。纳米三氧化钨与传统的半导体材料相比,禁带宽度较窄,在可见光条件下具有良好的光电响应性能,并且价格低廉、性能稳定、无害、无毒,可作为光催化剂,利用太阳光降解水中的有机污染物和空气中的废气,高效节能、清洁、无污染。然而,WO3的性能和实际应用与它的晶相、形态、尺寸、形貌、晶体缺陷以及表面性能紧密相关,而这些又主要取决于WO3的制备方法及制备条件。其中,多孔纳米片是一种带有空洞的二维结构,它具有较高的比表面积,表现出高度的各向异性和量子限域效应。当多孔纳米片形成介孔结构时,有利于介质的扩散,提高光催化效率。基于此,本发明提供了一种多孔WO3/C纳米片介孔复合光催化剂的制备方法。
发明内容
本发明目的在于提供一种多孔WO3/C纳米片介孔复合光催化剂的制备方法,解决现有WO3纳米片阵列材料光电性能不足,光催化效率低的技术问题。
本发明目的是通过以下技术方案来实现的:
一种多孔WO3/C纳米片介孔复合光催化剂的制备方法,将有机胺插层WO3·2H2O的杂化物加入瓷舟中,然后放入管式炉中,通入氮气,加热升温,保温反应,反应完后自然冷却至室温,即得到多孔WO3/C纳米片介孔复合光催化剂材料。
本发明多孔WO3/C纳米片介孔复合光催化剂的制备方法,通过在氮气中煅烧有机胺插层WO3·2H2O的无机/有机层状杂化物,在多孔WO3纳米片表面原位引入碳,构建多孔WO3/C纳米片介孔材料,,增加了比表面积和对气体的吸附能力,提高了可见光吸收、光致电荷分离效率,结果有利于电子与空穴的分离,提高反应效率和分离效率,从而增强了光催化性能。
本发明中,有机胺插层WO3·2H2O的杂化物为WO3·2H2O/正丙胺无机/有机层状杂化物、WO3·2H2O/正丁胺无机/有机层状杂化物、WO3·2H2O/正辛胺无机/有机层状杂化物和WO3·2H2O/十二胺无机/有机层状杂化物中的一种。
本发明中,加热升温速率为10℃-25℃/min,加热至400-600℃,反应时间为2-4h。
与现有技术相比,本发明具有以下有益效果:
(1)本发明方法制备的多孔WO3/C纳米片介孔复合光催化剂由C与多孔的WO3纳米片形成的介孔结构的复合材料,具有良好的光吸收性能和较大的比表面积,在光照下能够高效的转化氮气成硝酸根,具有较好的光催化氧化活性。
(2)本发明制备的多孔WO3/C纳米片介孔复合光催化剂光催化氧化氮气成为硝酸根的能力明显高于纯的多孔WO3纳米片介孔结构,可以作为一种可见光响应材料,在光催化转化氮方面具有很大的应用潜能。
(3)本发明多孔WO3/C纳米片介孔复合光催化剂的制备方法操作简便、条件温和、产率高,制备的材料具有较好的光催化分解水的性能,在光电转化方面具有很大的应用价值。
附图说明
图1为实施例1制备的多孔WO3/C纳米片介孔复合光催化剂材料的XRD图;
图2为本发明实施例1制备的多孔WO3/C纳米片介孔复合光催化剂材料的TEM图;
图3为本发明实施例1制备的多孔WO3/C纳米片介孔复合光催化剂材料SEM图;
图4为本发明实施例1制备的多孔WO3/C纳米片介孔复合光催化剂材料的紫外-可见漫反射光谱图;
图5为本发明实施例1制备的多孔WO3/C纳米片介孔复合光催化剂材料的吸附-解吸图;
图6为本发明实施例1制备的多孔WO3/C纳米片介孔复合光催化剂材料的光催化氧化N2成NO3 -的曲线图。
具体实施方式
以下结合具体的实施例对本发明作进一步的说明,以便本领域技术人员更好理解和实施本发明的技术方案。
实施例1
一种多孔WO3/C纳米片介孔复合光催化剂的制备方法,包括以下步骤:
将0.1gWO3·2H2O/正丙胺无机/有机层状杂化物加入瓷舟中,然后将瓷舟放入管式炉中,通入氮气。设定加热速率为10℃/min,加热时间为40min,加热至400℃,保温时间为2h。反应结束后让其自然冷却至室温,取出得到多孔WO3/C纳米片介孔复合光催化剂材料。
本实施例中多孔WO3/C纳米片介孔复合光催化剂材料的XRD图,如图1所示;多孔WO3/C纳米片介孔复合光催化剂材料的TEM图,如图2所示;多孔WO3/C纳米片介孔复合光催化剂材料在不同放大倍率下的SEM图,如图3所示,其中(a)60000倍(b)30000倍(c)10000倍(d)5000倍;多孔WO3/C纳米片介孔复合光催化剂材料的紫外-可见漫反射光谱图,如图4所示;多孔WO3/C纳米片介孔复合光催化剂材料的吸附-解吸图,如图5所示。
实施例2
一种多孔WO3/C纳米片介孔复合光催化剂的制备方法,包括以下步骤:
将0.5gWO3·2H2O/正丁胺无机/有机层状杂化物加入瓷舟中,然后将瓷舟放入管式炉中,通入氮气。设定加热速率为25℃/min,加热时间为40min,加热至600℃,,保温时间为4h。反应结束后让其自然冷却至室温,取出得到多孔WO3/C纳米片介孔复合光催化剂材料。
实施例3
一种多孔WO3/C纳米片介孔复合光催化剂的制备方法,包括以下步骤:
将0.2gWO3·2H2O/正辛胺无机/有机层状杂化物加入瓷舟中,然后将瓷舟放入管式炉中,通入氮气。设定加热速率为15℃/min,加热时间为40min,加热至500℃,保温时间为3h。反应结束后让其自然冷却至室温,取出得到多孔WO3/C纳米片介孔复合光催化剂材料。
实施例4
一种多孔WO3/C纳米片介孔复合光催化剂的制备方法,包括以下步骤:
将0.3gWO3·2H2O/十二胺无机/有机层状杂化物加入瓷舟中,然后将瓷舟放入管式炉中,通入氮气。设定加热速率为20℃/min,加热时间为40min,加热至600℃,保温时间为4h。反应结束后让其自然冷却至室温,取出得到多孔WO3/C纳米片介孔复合光催化剂材料。
称取实施例1制备的多孔WO3/C纳米片介孔复合光催化剂材料样品20mg倒入烧杯中,向其中加入120mL超纯水,超声30min。检查装置的气密性,将超声好的样品倒入气密性良好光反应器中,再次密封并检查气密性。用真空泵将反应器抽真空,然后用针管把氮气和氧气注入反应器中(比例为3:1),静置1h,打开氙灯稳流电源,把光反应器放到磁力搅拌机上搅拌,调整光源使光反应器置于光照中心。每隔半个小时取一次样,每次取8mL注入取样管中,在每次取样的时候适量补充氮气和氧气,保证光反应器中氮气与氧气的量充足,反应时间为3h。反应结束后将取出的液体样品送去离子色谱仪检测是否含有硝酸根离子。由标准溶液测定硝酸根浓度与峰面积的拟合曲线,测定样品的峰面积算出硝酸根浓度,最后作出时间与浓度的曲线,结果如图6所示。
由图1可见,b在23.08°、23.71°、24.09°、33.33°、34.02°处都有明显的衍射峰,分别对应WO3/C标准卡片(JCPDFCardNo.53-0433)中的(001)、(020)、(200)、(021)、(220),说明生成了WO3/C复合物。a是用作对照的纯的多孔WO3纳米介孔材料。
由图2可以看出WO3纳米片上有许多的孔洞,黑色的颗粒是碳,它与多孔WO3纳米片结合在一起形成了WO3/C复合物。
由图3中可见WO3·2H2O/丙胺无机/有机层状杂化物在氮气中烧结后产生WO3纳米片,纳米片与纳米片之间形成丰富的介孔结构,这种结构将具有较大的比表面积和孔隙率,能够提高光催化性能。
由图4可见WO3/正丙胺前驱体在300-500nm之间没有吸收,WO3粉末小于500nm范围有较大吸收,多孔WO3纳米片介孔结构吸收范围在450nm以下。多孔WO3/C纳米片介孔复合材料不但在紫外去有较大吸收,在整个可见光区均有较强吸收,这是由于碳修饰在多孔WO3/C纳米片上的结果。碳修饰增强了可见光区吸收,能够提高可见光的利用率,增强光催化活性。
由图5可见多孔WO3/C纳米片介孔结构具有较大的比表面积(5.5855m2/g),可能产生更多的活性位点,从而有利于提高复合材料的光催化性能。
由图6可见以多孔WO3/C纳米片介孔复合材料为催化剂,所产生的硝酸银产率持续上升,且在相同的反应时间内,硝酸银的产率始终高于纯的多孔WO3纳米片介孔材料,特别是反应到1.5h以后,多孔WO3/C纳米片介孔复合材料的催化效率还在上升且显著高于纯的多孔WO3纳米片介孔材料。这说明复合材料的光催化性能更好。
以上实施实例对本发明不同的实施过程进行了详细的阐述,但是本发明的实施方式并不仅限于此,所属技术领域的普通技术人员依据本发明中公开的内容,均可实现本发明的目的,任何基于本发明构思基础上做出的改进和变形均落入本发明的保护范围之内,具体保护范围以权利要求书记载的为准。
Claims (3)
1.一种多孔WO3/C纳米片介孔复合光催化剂的制备方法,其特征在于,将有机胺插层WO3·2H2O的杂化物加入瓷舟中,然后放入管式炉中,通入氮气,加热升温,保温反应,反应完后自然冷却至室温,即得到多孔WO3/C纳米片介孔复合光催化剂材料。
2.根据权利要求1所述多孔WO3/C纳米片介孔复合光催化剂的制备方法,其特征在于,有机胺插层WO3·2H2O的杂化物为WO3·2H2O/正丙胺无机/有机层状杂化物、WO3·2H2O/正丁胺无机/有机层状杂化物、WO3·2H2O/正辛胺无机/有机层状杂化物和WO3·2H2O/十二胺无机/有机层状杂化物中的一种。
3.根据权利要求1或2所述多孔WO3/C纳米片介孔复合光催化剂的制备方法,其特征在于,加热升温速率为10℃-25℃/min,加热至400-600℃,反应时间为2-4h。
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